CN103922343B - Silicon carbide cutting blade material de_ironing refinement method - Google Patents
Silicon carbide cutting blade material de_ironing refinement method Download PDFInfo
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- CN103922343B CN103922343B CN201410101307.0A CN201410101307A CN103922343B CN 103922343 B CN103922343 B CN 103922343B CN 201410101307 A CN201410101307 A CN 201410101307A CN 103922343 B CN103922343 B CN 103922343B
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- silicon carbide
- cutting blade
- carbide powder
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Abstract
The invention discloses a kind of silicon carbide cutting blade material de_ironing refinement method, be intended to solve that existing silicon carbide cutting blade material de_ironing refinement method cost is high, efficiency is low, easily cause the technical problem of environmental pollution.Comprise the following steps: by cover through thunder pulverizer pulverize after silicon carbide micro-powder mix pulping with water; Ultrasonic oscillation process is carried out to the silicon carbide powder slip of gained; Then sieved by spin vibration sieve; Again the slip of gained is introduced successively the two-stage electromagnetic deironing apparatus be in series, removing iron contamination wherein, obtain the silicon carbide powder slip after purifying.Silicon carbide cutting blade material quality product after adopting the method to purify can meet Technical specifications, stable processing technique, significantly can shorten the production cycle, enhance productivity and environmental protection and energy saving.
Description
Technical field
The present invention relates to silicon carbide cutting blade material production technical field, be specifically related to a kind of silicon carbide cutting blade material de_ironing refinement method.
Background technology
Silicon carbide has very high hardness, chemical stability and certain toughness, is widely used in manufacturing in bonded abrasive tool, coated abrasive article and free grinding technique.Along with the increase of photovoltaic market sun power crystal silicon wafer cutting edge material demand, the quality requirements of silicon carbide cutting blade material is significantly improved, also more and more higher to the purity requirement of silicon carbide micro-powder, the purification therefore in silicon carbide cutting blade material preparation process becomes an important production process.Become large ingot after silicon carbide smelting, can iron contamination be introduced in follow-up Mechanical Crushing and pulverizing process, thus affect the quality of cutting blade material, therefore need the iron contamination removed wherein.
The method of purification of silicon carbide cutting blade material mainly acid adding deironing in prior art, i.e. pickling, due to silicon carbide not with any acid-base reaction, the object of pickling is removing metallic iron and ferric oxide, and a part of calcium oxide, magnesium oxide, aluminum oxide and graphite.Can generate acid salt in pickling reaction, they can be dissolved in water, and used water is rinsed and discharged.But because the particle of micro mist is too little, not allowing to adopt the method for continuous flushing, just can change water and rinsing after normally leaving standstill clarification for some time when rinsing, often rinsing once must once settling process next time.Silicon carbide cutting blade material pickling iron removal not only can produce a large amount of waste water, easy contaminate environment, and the cost of business processes waste water drops into also corresponding increase; And it is long to wash required time in acid cleaning process, the overall production cycle is extended, and production efficiency is low; And pickling need dilute the reacted sour water of acid adding with a large amount of water, production cost is high, and water resource waste is serious.Therefore, in current photovoltaic industry under the quality requirements of silicon carbide cutting blade material, a kind of silicon carbide cutting blade material physics de_ironing refinement method of inventing energy-conserving and environment-protective is necessary.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of high and silicon carbide cutting blade material de_ironing refinement method of energy-conserving and environment-protective of purification efficiency.
For solving the problems of the technologies described above, silicon carbide cutting blade material de_ironing refinement method of the present invention comprises the following steps:
(1) pulping: the silicon carbide micro-powder of size range between 14.00 μm ~ 4.80 μm cover pulverizer pulverizing through thunder after is mixed with water, stirs 20 ~ 40 minutes, form the silicon carbide powder slip that mass percent concentration is 33% ~ 40%;
(2) ultrasonic oscillation: the silicon carbide powder slip of step (1) gained being placed in frequency is shake process 20 ~ 30 minutes under 25 ~ 60KHz ultrasonic wave;
(3) sieve removal of impurities: sieved by the silicon carbide powder slip of step (2) gained, remove fiber, floss, graphite granule and macrobead silicon carbide powder impurity wherein;
(4) electromagnetism deironing: by the silicon carbide powder slip of step (3) gained with 3.5 ~ 4m
3the input speed of/h introduces the two-stage electromagnetic deironing apparatus be in series successively, removing iron contamination wherein, obtains the silicon carbide powder slip after purifying.
In technique scheme, the silicon carbide powder slip that mass percent concentration is 33 ~ 40% is formed after step (1) pulping, the powder slip of this concentration is conducive to reaching better removal of impurities and de-ferrous effect in follow-up treating processes, easily block the screen cloth of screening removal of impurities during excessive concentration, reduce the working efficiency of screening plant and ferromagnetic substance removing device; Screening removal of impurities and the time needed for electromagnetism deironing can be caused when concentration is too low to increase, efficiency reduces and the waste of water resources.The effect that step (2) carries out ultrasonic oscillation process is that the micro mist in slip and impurity are uniformly dispersed more fully, is conducive to improving follow-up screening removal of impurities and electromagnetism de-ironing efficiency, reaches better refining effect.The electromagnetism iron removal of step (4) makes slip successively by the two-stage electromagnetic deironing apparatus of series connection, avoids and uses chemical method deironing and produce a large amount of useless water problem, energy-conserving and environment-protective, and can reach good de-ferrous effect, enhances productivity.
Preferably, step (3) described screening process is: the silicon carbide powder slip of step (2) gained is introduced spin vibration sieve and sieves, the screen cloth of described spin vibration sieve is 360-400 order; Described spin vibration sieve is ability of swimming spin vibration sieve; Or described spin vibration sieve is ultrasonic wave spin vibration sieve.
Preferably, also comprising the following steps: after step (3), before step (4) that the silicon carbide powder slip after step (3) screening is collected in the slurry tank of vertical position higher than ferromagnetic substance removing device opening for feed by a., produce difference of altitude, then be introduced in ferromagnetic substance removing device.
Preferably, in described electromagnetism iron removal, silicon carbide powder slip by a ferromagnetic substance removing device time used is: feed time 120 seconds, 10 seconds blowing time, scavenging period 15 seconds.
Preferably, described ferromagnetic substance removing device is Full-automatic electromagnetic pulp deferrization device, and its solenoid magnetic field is 20000GS, and coil current is 90A.
The beneficial effect of silicon carbide cutting blade material de_ironing refinement method of the present invention is adopted to be:
1. the silicon carbide cutting blade material quality product after purifying can meet Technical specifications, and after de_ironing refinement of the present invention, silicon carbide cutting blade material just directly can enter lower road work program, stable processing technique;
2. significantly can shorten the production cycle, enhance productivity;
3. can reduce the water consumption of purification phase, saving water resource, reduces costs;
4. do not re-use sulfuric acid reaction, energy-conserving and environment-protective, meet national requirements for environmental protection, free from environmental pollution.
For concrete operation step of the present invention and flow process, further detailed description will be made by reference to the accompanying drawings below.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of silicon carbide cutting blade material de_ironing refinement method of the present invention.
Fig. 2 is two-stage electromagnetic iron removal schematic diagram of the present invention.
Wherein, 1 is slurry tank; 2 is one-level deironing apparatus; 3 is secondary deironing apparatus; 4 is collecting tank.
Embodiment
The process flow sheet of silicon carbide cutting blade material de_ironing refinement method of the present invention as shown in Figure 1, comprises the following steps:
First by cover through thunder pulverizer pulverize after the silicon carbide micro-powder of size range between 14.00 μm ~ 4.80 μm mix with water, stir 20 ~ 40 minutes, formation mass percent concentration be 33% ~ 40% silicon carbide powder slip; Then the silicon carbide powder slip of gained being placed in frequency is shake process 20 ~ 30 minutes under 25 ~ 60KHz ultrasonic wave; The material dispersion of reuniting in slip is opened; Again the silicon carbide powder slip of gained is introduced spin vibration sieve to sieve, the screen cloth of described spin vibration sieve is 360 ~ 400 orders, removes the impurity such as fiber, floss, graphite granule and the macrobead silicon carbide powder (i.e. the silicon carbide powder particle of particle diameter more than 40 μm) in slip; Again by the silicon carbide powder slip of gained with 3.5 ~ 4m
3the input speed of/h introduces the two-stage electromagnetic deironing apparatus (as shown in Figure 2) be in series successively, removing iron contamination wherein, obtains the silicon carbide powder slip after purifying.
Silicon carbide powder slip after screening is collected in the slurry tank of vertical position higher than ferromagnetic substance removing device opening for feed, produces difference of altitude, then be introduced in ferromagnetic substance removing device.Being conducive to slip like this leans on the effect of self gravitation to enter in ferromagnetic substance removing device, can reduce propulsion source, cost-saving.In electromagnetism iron removal, silicon carbide powder slip by a ferromagnetic substance removing device time used is: feed time 120 seconds, 10 seconds blowing time, scavenging period 15 seconds.Described ferromagnetic substance removing device is Full-automatic electromagnetic pulp deferrization device, and model is XYDC-Z12K, and its solenoid magnetic field is 20000GS, and coil current is 90A.
Silicon carbide micro-powder impurities Fe after de_ironing refinement of the present invention
2o
3content meet the requirement of industry standard, the silicon carbide cutting blade material after de_ironing refinement directly can enter lower road production process and carry out size classification.
In the fragmentation and pulverizing process of silicon carbide, the iron contamination content of silicon carbide cutting blade material is generally 0.35 ~ 0.6%, and the chemical composition of compound before purification after silicon carbide pulverizing is as shown in table 1 below.
Silicon carbide micro-powder impurities Fe after two-stage de_ironing refinement of the present invention
2o
3content be 0.08 ~ 0.15%, meet the requirement of industry standard, the silicon carbide cutting blade material after de_ironing refinement directly can enter lower road production process and carry out size classification.Chemical composition industry standard in silicon carbide cutting blade material sees the following form 2.
The following examples are only used to describe the present invention in detail, and limit the scope of the invention never in any form.
Embodiment 1: by cover through thunder pulverizer pulverize after the silicon carbide micro-powder of size range between 14.00 μm ~ 4.80 μm and water by 40% concentration dilution pulping, first add water and feed in raw material again, stir and within 30 minutes, make meal fully mix with water, pulping tank pulping 1 ton.Then the silicon carbide powder slip of gained being placed in frequency is shake process 20 minutes under 60KHz ultrasonic wave.Again the slip after ultrasonic oscillation process is pumped in the opening for feed distributor of ability of swimming spin vibration sieve, the impurity such as fiber, floss, mao mao, graphite granule, macrobead silicon carbide powder in slip is removed by screening, wherein sieve machine screen is 363 orders, and the impurity on 10 hours cleaning screen clothes.By collecting in the slurry tank of vertical position higher than ferromagnetic substance removing device opening for feed by the silicon carbide powder slip after screening removal of impurities, producing difference of altitude, finally it being introduced successively the two-stage electromagnetic deironing apparatus be in series, removing iron contamination wherein.In electromagnetism iron removal, silicon carbide powder slip by a ferromagnetic substance removing device time used is: feed time 120 seconds, 10 seconds blowing time, scavenging period 15 seconds.Silicon carbide micro-powder impurities Fe after two-stage de_ironing refinement
2o
3content be 0.08-0.15%, meet the requirement of industry standard, the silicon carbide cutting blade material after de_ironing refinement directly can enter lower road production process and carry out size classification.
Ferromagnetic substance removing device used is Full-automatic electromagnetic pulp deferrization device, and model is XYDC-Z12K, and its magnetic coil produces high-intensity magnetic field in galvanization, is picked up by the ironware in non-magnetic material, reaches purification object.The solenoid magnetic field of this equipment is 20000GS, and coil current is 90A.
Embodiment 2: adopt the method identical with embodiment 1 to carry out silicon carbide cutting blade material de_ironing refinement, difference is, pulping concentration is 35%, and churning time is 25 minutes; The ultrasonic oscillation process of ultrasonic oscillation process employing 50KHz 30 minutes.
Embodiment 3: adopt the method identical with embodiment 1 to carry out silicon carbide cutting blade material de_ironing refinement, difference is, the ultrasonic oscillation process of ultrasonic oscillation process employing 30KHz 20 minutes; Spin vibration sieve used is ultrasonic wave spin vibration sieve, while screening process medium and low frequency revolves vibration, be superimposed with ultrasonic vibration, realize effective combination of ultrasonic oscillation and vibratory screening apparatus, the material in slip can be made more to disperse, the separation of further quickening aggregate, also can prevent mesh from blocking, realize better screening effect.
Plant and instrument involved in the above-described embodiments if no special instructions, is routine instrument device; Involved industrial raw material if no special instructions, is commercially available regular industrial raw material.
Silicon carbide cutting blade material electromagnetism de_ironing refinement process de-ironing efficiency of the present invention is at 2.5t/h, and de_ironing refinement efficiency improves greatly; Pulping water consumption is 3m
3/ t, can saving water resource in a large number, reduces production cost, and there is not water pollution problems.
Adopt silicon carbide cutting blade material de_ironing refinement method of the present invention, compared with existing chemical removal of iron method of purification:
1. after electromagnetism de_ironing refinement of the present invention, the quality product of silicon carbide cutting blade material is well positioned to meet Technical specifications, i.e. Fe
2o
3content≤0.15%, stable processing technique;
2. significantly can shorten the production cycle, enhance productivity, 2.5t/h can be increased to by the 0.07t/h of chemical purification;
3. can reduce the water consumption of purification phase, saving water resource, reduces costs, can by the 20m of chemical purification
3/ t is reduced to 3-4m
3/ t;
4. do not re-use sulfuric acid and carry out pickling reaction, energy-conserving and environment-protective, free from environmental pollution, save production cost.
Silicon carbide cutting blade material de_ironing refinement method of the present invention can improve quality, the reduction production cost of silicon carbide cutting blade material product, effectively can enhance productivity and environmental protection and energy saving, be suitable for large-scale promotion and use.
In conjunction with the accompanying drawings and embodiments the present invention is described in detail above, but, person of ordinary skill in the field can understand, under the prerequisite not departing from present inventive concept, each design parameter in above-described embodiment can also be changed, form multiple specific embodiment, be common variation range of the present invention, describe in detail no longer one by one at this.
Claims (1)
1. a silicon carbide cutting blade material de_ironing refinement method, is characterized in that, comprise the following steps:
(1) pulping: the silicon carbide micro-powder of size range between 14.00 μm ~ 4.80 μm cover pulverizer pulverizing through thunder after is mixed with water, stirs 20 ~ 40 minutes, form the silicon carbide powder slip that mass percent concentration is 33% ~ 40%;
(2) ultrasonic oscillation: the silicon carbide powder slip of step (1) gained being placed in frequency is shake process 20 ~ 30 minutes under 25 ~ 60KHz ultrasonic wave;
(3) removal of impurities is sieved: the silicon carbide powder slip of step (2) gained is introduced spin vibration sieve and sieves, remove fiber, floss, graphite granule and macrobead silicon carbide powder impurity wherein, described spin vibration sieve is ability of swimming spin vibration sieve or ultrasonic wave spin vibration sieve, and the screen cloth of described spin vibration sieve is 360-400 order; And then the silicon carbide powder slip after screening is collected in the slurry tank of vertical position higher than ferromagnetic substance removing device opening for feed;
(4) electromagnetism deironing: by the silicon carbide powder slip of step (3) gained with 3.5 ~ 4m
3the input speed of/h introduces the two-stage electromagnetic deironing apparatus be in series successively, removing iron contamination wherein, obtains the silicon carbide powder slip after purifying; In this electromagnetism iron removal, silicon carbide powder slip by a ferromagnetic substance removing device time used is: feed time 120 seconds, 10 seconds blowing time, scavenging period 15 seconds, described ferromagnetic substance removing device is Full-automatic electromagnetic pulp deferrization device, its solenoid magnetic field is 20000GS, and coil current is 90A.
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| CN104401997B (en) * | 2014-11-18 | 2016-08-24 | 河南易成新能源股份有限公司 | The processing means of high ferro silicon carbide micro-powder and processing method |
| CN105668570A (en) * | 2016-01-14 | 2016-06-15 | 宝兴易达光伏刃料有限公司 | Preparation method of silicon wafer cutting edge material |
| CN105597928B (en) * | 2016-03-21 | 2017-05-03 | 平顶山市国邦新材料有限公司 | Silicon carbide powder production system |
| CN106430210A (en) * | 2016-08-31 | 2017-02-22 | 江西恩克新材料股份有限公司 | Method for removing iron and silicon impurities in silicon carbide micropowder for crystalline silicon wire cutting |
| KR102270052B1 (en) * | 2019-09-03 | 2021-06-28 | 주식회사 케이씨인더스트리얼 | PREPARATION METHOD OF HIGH PURITY SiC POWDER |
| US11718532B2 (en) * | 2018-12-27 | 2023-08-08 | Kcindustrial Co., Ltd. | Preparation method of high purity SiC powder |
| DE102020102512A1 (en) * | 2020-01-31 | 2021-08-05 | ESK - SIC GmbH | Process for separating impurities from silicon carbide and purified silicon carbide powder - US Pat |
| CN113548666B (en) * | 2021-08-16 | 2023-01-31 | 东北大学 | Iron removal process for submicron silicon carbide powder |
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